Hermetically sealed molecular spectroscopy cell with dual wafer bonding

ABSTRACT

A method includes forming a plurality of layers of an oxide and a metal on a substrate. For example, the layers may include a metal layer sandwiched between silicon oxide layers. A non-conductive structure such as glass is then bonded to one of the oxide layers. An antenna can then be patterned on the non-conductive structure, and a cavity can be created in the substrate. Another metal layer is deposited on the surface of the cavity, and an iris is patterned in the metal layer to expose the one of the oxide layers. Another metal layer is formed on a second substrate and the two substrates are bonded together to thereby seal the cavity.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. patent application Ser. No.15/698,346 filed Sep. 7, 2017, which is fully incorporated herein byreference.

BACKGROUND

Various applications may include a sealed chamber formed in asemiconductor structure. In one particular application, a chip-scaleatomic clock may include a selected vapor at a low pressure in a sealedchamber. Forming such structures can be a challenge.

SUMMARY

In one embodiment, a method includes forming a plurality of layers of anoxide and a metal on a substrate. For example, the layers may include ametal layer sandwiched between silicon oxide layers. A non-conductivestructure such as glass is then bonded to one of the oxide layers. Anantenna can then be patterned on the non-conductive structure, and acavity can be created in the substrate. Another metal layer is depositedon the surface of the cavity, and an iris is patterned in the metallayer to expose the one of the oxide layers. Another metal layer isformed on a second substrate and the two substrates are bonded togetherto thereby seal the cavity. The method also may include the depositionor bonding of further dielectric and metal layers and their subsequentpatterning on the topmost surface to improve the radio frequency (RF)performance of antenna, transmission line structures, andelectromagnetic bandgap structures.

In another embodiment, a device includes a first substrate that includesa cavity. The device also includes a first oxide layer on a surface ofthe first substrate, a first metal layer on a surface of the first oxidelayer opposite the first substrate, and a second oxide layer on asurface of the first metal layer opposite the first oxide layer. Thedevice further includes a non-conductive structure bonded to a surfaceof the second oxide layer opposite the first metal layer, a firstantenna patterned on a surface of the non-conductive structure oppositethe second oxide layer, and a second substrate bonded to the firstsubstrate to thereby seal the cavity. The cavity in this embodimentextends from an interface between the first and second substrates to thesecond oxide layer.

Yet another embodiment is directed to a device that includes a firstsemiconductor substrate in which a cavity has been formed. The devicealso includes a first oxide layer on a surface of the firstsemiconductor substrate, a first metal layer on a surface of the firstoxide layer opposite the first semiconductor substrate, and a secondoxide layer on a surface of the first metal layer opposite the firstoxide layer. The device further includes a glass sheet bonded to asurface of the second oxide layer opposite the first metal layer, firstand second antennas patterned on a surface of the glass sheet oppositethe second oxide layer, a second semiconductor substrate bonded to thefirst semiconductor substrate to thereby seal the cavity, and atransceiver electrically coupled to the first and second antennas andconfigured to inject a transmit signal into the cavity through the firstantenna. The cavity contains dipolar molecules and has an internalpressure of less than, for example, 0.15 mbars. The transceiver isconfigured also to generate an error signal based on the transmit signaland a receive signal from the second antenna and dynamically adjust afrequency of the transmit signal based on the error signal.

BRIEF DESCRIPTION OF THE DRAWINGS

FIGS. 1A-1I illustrate a sequence of processing operations in oneembodiment to form a hermetically sealed cavity.

FIG. 2 illustrates a method flow chart to form a hermetically sealedcavity in accordance with various embodiments.

FIG. 3 shows a cross-sectional view of the hermetically sealed cavity ofvarious embodiments.

FIG. 4 shows a block diagram for a clock generator in accordance withvarious embodiments.

DETAILED DESCRIPTION OF EXAMPLE EMBODIMENTS

In this description, the term “couple” or “couples” means either anindirect or direct wired or wireless connection. Thus, if a first devicecouples to a second device, that connection may be through a directconnection or through an indirect connection via other devices andconnections. Also, in this description, the recitation “based on” means“based at least in part on.” Therefore, if X is based on Y, then X maybe a function of Y and any number of other factors.

The disclosed embodiments of the present disclosure include techniquesto fabricate a hermetically sealed cavity in a substrate. A structurecontaining a substrate with the cavity may be used in numerousapplications. One illustrative use is as a millimeter wave chip scaleatomic clock. The cavity may contain a plurality of dipolar molecules(e.g., water molecules) at a relatively low pressure. For someembodiments, the pressure may be approximately 0.1 mbarr for watermolecules. If argon molecules were used, the pressure may be severalatmospheres. The hermetically sealed cavity may contain selected dipolarmolecules at a pressure chosen to optimize the amplitude of a signalabsorption peak of the molecules detected at an output of the cavity. Anelectromagnetic signal may be injected through aperture into the cavity.Through closed-loop control, the frequency of the signal is dynamicallyadjusted to match the frequency corresponding to the absorption peak ofthe molecules in the cavity. The frequency produced by quantum rotationof the selected dipolar molecules may be unaffected by circuit aging andmay not vary with temperature or other environmental factors.

While a variety of materials and manufacturing operations can beemployed, one illustrative method may include forming a plurality oflayers of an oxide and a metal on a substrate. For example, the layersmay include a metal layer sandwiched between silicon oxide layers. Anon-conductive structure such as glass is then bonded to one of theoxide layers. An antenna can then be patterned on the non-conductivestructure, and a cavity can be created in the substrate. Another metallayer is deposited on the surface of the cavity, and an iris ispatterned in the metal layer to expose the one of the oxide layers.Another metal layer is formed on a second substrate and the twosubstrates are bonded together to thereby seal the cavity.

FIGS. 1A-1I illustrate a sequence of process steps to fabricate ahermetically sealed cavity in accordance with an embodiment. At FIG. 1A,a first oxide layer 102 is formed on a first substrate 120. A firstmetal layer 104 is formed on a surface of the first oxide layer 102opposite the first substrate 120. The first metal layer 104 may comprisecopper or another suitable metal. A second oxide layer 106 is formed ona surface of the first metal layer 104 opposite the first oxide layer102. The oxide layers may comprise silicon oxide and layers 102-106 maybe formed in accordance with any suitable semiconductor processoperations. The substrate 120 is a semiconductor substrate (e.g.,silicon) in some embodiments, but can be other than a semiconductorsubstrate in other embodiments, such as a ceramic material or a metalliccavity.

At FIG. 1B, a non-conductive structure 108 is bonded to a surface of thesecond oxide layer 106 opposite the first metal layer 104. In oneexample, the non-conductive structure comprises glass (e.g., 130micrometers thick), but can include other types of materials such asceramic or silicon in other embodiments. The process to bond thenon-conductive structure 108 to the second oxide layer 106 may comprisean anodic, fusion, eutectic solder, transition liquid phase (TLP),cofiring, or other suitable bonding processes.

FIG. 1C illustrates that an antenna 110 has been patterned on a surfaceof the non-conductive structure 108. The antenna 110 comprises aconductive material such as copper or gold and an electrical signal canbe provided to the antenna or received from the antenna. In someembodiments, one antenna is used to both transmit and receive signals.In other embodiments, a pair of antennas is patterned on thenon-conductive structure 108, and one antenna is used to inject a signalinto the cavity and another antenna is used to receive a signal from thecavity. In such examples, the antennas may be located at or nearopposite ends of the cavity. FIG. 1D illustrates that an oxide layer 115is formed on a surface of the non-conductive structure 108. Oxide layer115 also covers the antenna 110 and functions to protect the antennaduring subsequent process operations. FIG. 1D also illustrates that acavity 125 has been created in the substrate 120. The cavity 125 may bewet etched into the substrate 120 using a suitable wet etchant such aspotassium hydroxide (KOH) or tetramethylammonium hydroxide (TMAH).Alternatively, the cavity 125 can be formed by way of reactive-ionetching (RIE), deep reactive-ion etching (DRIE), or isotropic etching.The cavity 125 is etched from the surface 126 of the substrate 120opposite the first oxide layer 102 to the first oxide layer 102, therebyexposing a portion of the first oxide layer 102. FIG. 1E illustratesthat another metal layer 130 has been deposited on a surface of thesubstrate 120 opposite the first oxide layer 102. The metal layer 130also is deposited in the cavity 125 as shown and may be sputterdeposited (e.g., 40 nm TaN per micrometer of copper).

FIG. 1F illustrates that an iris 140 is created in the metal layer 130within the cavity 125. The iris 140 is patterned (e.g., by wet etching,dry etching, liftoff, etc.) in the metal layer 130 and exposes at leasta portion of the second oxide layer 130. The iris 140 permits the RFenergy from the incident radio frequency (RF) signal provided by theantenna 110 is able to penetrate through the iris 140 and into thecavity 125, and back out again through another iris formed in the cavityand associated with another antenna (noted above).

FIG. 1G shows a second substrate 150 and a metal layer 152 formedthereon. The substrate 150 may comprise the same or different materialas substrate 120. In one example, the substrate 150 comprises asemiconductor substrate such as a silicon wafer, but can be other than asemiconductor material in other examples. FIGS. 1H and 1I illustratethat bonding structures 155 are deposited and patterned on either orboth of the substrates 120 and 150. In one example, the bondingstructures comprise a gold, aluminum, silicon or other types of materialthat form an alloy when heated to a suitable temperature. FIG. 1Iillustrates the resulting device which includes a hermetically sealedcavity. Dipolar molecules (e.g., water molecules) may be trapped insidethe cavity 125 and at an internal pressure of less than approximately0.15 mbars (e.g., 0.1 mbars).

The flow chart of FIG. 2 illustrates a method in accordance with anexample. The operations may be performed in the order shown, or in adifferent order. Further, the operations may be performed sequentially,or two or more of the operations may be performed concurrently.

At 202, the method includes forming a first oxide layer on a firstsubstrate (e.g., a semiconductor substrate such as a wafer). Theillustrative method then includes (204) forming a first metal layer(e.g., copper) on a surface of the first oxide layer opposite the firstsubstrate. At 206, the method includes forming a second oxide layer on asurface of the first metal layer opposite the first oxide layer. Assuch, a metal layer is created sandwiched between to oxide layers.

At 208, the method includes bonding a non-conductive structure (e.g.,glass) to a surface of the second oxide layer opposite the first metallayer, and at 210 patterning an antenna (e.g., antenna 110) on thenon-conductive structure. A cavity is then created at 212 (e.g., by awet etching process) in the substrate. The cavity extends from onesurface of the substrate to the opposing surface (and thus to the firstoxide layer).

At 214, a second metal layer is deposited in the interior surface of thecavity and on a surface of the first substrate outside the cavity. At216, the method includes patterning an iris in the second metal layer toexpose the second oxide layer. A metal layer is formed (218) on a secondsubstrate (e.g., another semiconductor wafer) and the first and secondsubstrates are then bonded together at 220 to thereby seal the cavity.In one embodiment, the substrates are bonded via eutectic bonds, orother suitable bonding techniques.

FIG. 3 shows a cross-sectional view of a structure in accordance withthe disclosed embodiments. The structure may comprise a millimeter wavechip scale atomic clock. Substrate 120 is shown bonded to substrate 150with a hermetically sealed cavity 125 formed in the substrate 120 andsealed at least in part by substrate 150. The non-conductive structure(e.g., glass) 108 is shown bonded to the substrate 120. A launchstructure 295 may comprise the antenna 110 described above and also atransmission line, and electromagnetic energy is permitted to passthrough the non-conductive structure 108 from the launch structure 295into the cavity 125. An electronic bandgap (EBG) structure 290 also isshown deposited and patterned on a surface of the non-conductivestructure 108. In operation, the EBG structure 290 attenuateselectromagnetic wave coupling along the outer surface of thenon-conductive structure 108 between the antennas. The EBG structure 290helps to force the energy from the input signal received through anantenna (e.g., antenna 110) into the cavity 125. Layer 104 provides acommon ground plane for all RF structures external to the cavity 125. Inaddition, it limits propagation of waves travelling in layer 120. Thedimensions of the waveguide, antenna, EBG, and size and positioning ofthe iris 140 are all design considerations based on the chosen molecularspecies inside the cavity and the wavelength of the interrogationwaveform within the cavity. The required bandwidth of the structuredepends upon the fabrication tolerances achievable in manufacturing.

FIG. 4 shows a block diagram for a clock generator 500 in accordancewith various embodiments. The clock generator 500 is a millimeter waveatomic clock that generates a reference frequency based on the frequencyof quantum rotation of selected dipolar molecules contained in ahermetically sealed cavity 102 formed in semiconductor material. Thereference frequency produced by quantum rotation of the selected dipolarmolecules is unaffected by circuit aging and does not vary withtemperature or other environmental factors.

The clock generator 500 of FIG. 4 includes a vapor cell 505 formed inthis example from substrates as described above. The cell 505 includes acavity 508 with a sealed interior enclosing a dipolar molecule materialgas, for example, water (H₂O) or any other dipolar molecule gas at arelatively low gas pressure inside the cavity 125. Non-limiting examplesof suitable electrical dipolar material gases include water,acetonitrile (CH₃CN) and hydrogen cyanide (HCN). As shown in FIG. 6, theclock generator 500 further includes a transceiver 600 with a transmitoutput 633 for providing an electrical transmit signal (TX) to the vaporcell 505, as well as a receiver input 638 for receiving an electricalinput signal (RX) from the vapor cell 525. The rotational transitionvapor cell 525 does not require optical interrogation, and insteadoperates through electromagnetic interrogation via the transmit andreceive signals (TX, RX) provided by the transceiver 600.

The sealed cavity 508 includes a conductive interior cavity surface, aswell as first and second non-conductive apertures 515 and 517 formed inthe interior cavity surface for providing an electromagnetic fieldentrance and an electromagnetic field exit, respectively. In oneexample, the apertures 515, 517 magnetically couple into the TE10 modeof the cavity 508. In other examples, the apertures 515, 517 excitehigher order modes. First and second conductive coupling structure 520and 525 are formed on an outer surface of the vapor cell 505 proximatethe first and second non-conductive aperture 515 and 517, respectively.The coupling structures 520, 525 may be the antenna(s) described aboveand may comprise a conductive strip formed on a surface of one of thesubstrates forming the cell 505. Each coupling structure 520, 525 mayoverlie and cross over the corresponding non-conductive aperture 515,517 for providing an electromagnetic interface to couple a magneticfield in to (based on the transmit signal TX from the transceiver output633) the cavity 508 or from the cavity to the transceiver RX input 638The proximate location of the conductive coupling structures 520, 525and the corresponding non-conductive apertures 515, 525 advantageouslyprovides electromagnetically transmissive paths through the second orupper substrate 106, which can be any electromagnetically transmissivematerial.

The transceiver circuit 600 in certain implementations is implemented onor in an integrated circuit (not shown), to which the vapor cell 505 iselectrically coupled for transmission of the TX signal via the output633 and for receipt of the RX signal via the input 638. The transceiver600 is operable when powered for providing an alternating electricaloutput signal TX to the first conductive coupling structure 520 forcoupling an electromagnetic field to the interior of the cavity 508, aswell as for receiving the alternating electrical input signal RX fromthe second conductive coupling structure 525 representing theelectromagnetic field received from the cavity 508. The transceivercircuit 600 is operable for selectively adjusting the frequency of theelectrical output signal TX in order to reduce the electrical inputsignal RX by interrogation to operate the clock generator 500 at afrequency which substantially maximizes the molecular absorption throughrotational motor state transitions, and for providing a reference clocksignal REF_CLK at the frequency of the TX output signal.

In certain examples, the transceiver 600 includes a signal generator 602with an output 633 electrically coupled with the first conductivecoupling structure 520 for providing the alternating electrical outputsignal TX, and for providing the reference clock signal REF_CLK at thecorresponding transmit output frequency. The transceiver 600 alsoincludes a lock-in amplifier circuit 606 with an input 638 coupled fromthe second conductive coupling structure 525 for receiving the RXsignal. The lock-in amplifier operates to provide an error signal ERRrepresenting a difference between the RX signal and the electricaloutput signal TX. In one example, the lock-in amplifier 606 provides theerror signal ERR as an in-phase output, and the error signal ERR is usedas an input by a loop filter 604 to provide a control output signal (CO)to the signal generator 602 for selectively adjusting the TX outputsignal frequency to maintain this frequency at a peak absorptionfrequency of the dipolar molecular gas inside the sealed interior of thecavity 508. In some examples, the RF power of the TX and RX loop iscontrolled so as to avoid or mitigate stark shift affects.

The electromagnetic coupling via the non-conductive apertures 520, 525and corresponding conductive coupling structures 515, 517 facilitateselectromagnetic interrogation of the dipolar gas within the cell cavity508. In one non-limiting form of operation, the clock generator 500operates with the signal generator 602 transmitting alternating current(AC) TX signals at full transmission power at various frequencies withina defined band around a suspected quantum absorption frequency at whichthe transmission efficiency of the vapor cell 505 is minimal (absorptionis maximal). For example, the quantum absorption frequency associatedwith the dipolar water molecule is 183.31 GHz. When the system operatesat the quantum frequency, a null or minima is detected at the receivervia the lock-in amplifier 606, which provides the error signal ERR tothe loop filter 604 for regulation of the TX output signal frequency viathe control output CO signal provided to the signal generator 602. Therotational quantum frequency of the dipolar molecule gas in the vaporcell cavity 508 is generally stable with respect to time (does notdegrade or drift over time), and is largely independent of temperatureand a number of other variables.

In one embodiment, the signal generator 602 initially sweeps thetransmission output frequency through a band known to include thequantum frequency of the cell 505 (e.g., transitioning upward from aninitial frequency below the suspected quantum frequency, or initiallytransitioning downward from an initial frequency above the suspectedquantum frequency, or other suitable sweeping technique or approach).The transceiver 600 monitors the received energy via the input 638coupled with (e.g., electrically connected to) the second conductivecoupling structure 525 in order to identify the transmission frequencyassociated with peak absorption by the gas in the cell cavity 508 (e.g.,minimal reception at the receiver). Once the quantum absorptionfrequency is identified, the loop filter 604 moves the source signalgenerator transmission frequency close to that absorption frequency(e.g., 183.31 GHz), and modulates the signal at a very low frequency toregulate operation around the null or minima in the transmissionefficiency representing the ratio of the received energy to thetransmitted energy. The loop filter 604 provides negative feedback in aclosed loop operation to maintain the signal generator 602 operating ata TX frequency corresponding to the quantum frequency of the cavitydipolar molecule gas.

In steady state operation, the lock-in amplifier 606 and the loop filter604 maintain the transmitter frequency at the peak absorption frequencyof the cell gas. In one non-limiting example, the loop filter 604provides proportional-integral-derivative (PID) control using aderivative of the frequency error as a control factor for lock-indetection and closed loop regulation. At the bottom of the null in atransmission coefficient curve, the derivative is zero and the loopfilter 604 provides the derivative back as a direct current (DC) controloutput signal CO to the signal generator 602. This closed loop operatesto keep the signal generator transmission output frequency at the peakabsorption frequency of the cell gas using lock-in differentiation basedon the RX signal received from the cell 508. The REF_CLK signal from thesignal generator 602 is the TX signal clock and can be provided to othercircuitry such as frequency dividers and other control circuitsrequiring use of a clock.

Modifications are possible in the described embodiments, and otherembodiments are possible, within the scope of the claims.

What is claimed is:
 1. A device, comprising: a first substrate havingopposite first and second sides, a cavity extending from the second sideof the first substrate through the first substrate to the first side ofthe first substrate; a first oxide layer on the first side of the firstsubstrate; a metal layer on the first oxide layer; a second oxide layeron the metal layer, the cavity extending from the first side of thefirst substrate through the first oxide layer and through the metallayer to the second oxide layer; an insulative layer on the second oxidelayer; an antenna on the insulative layer; a second substrate; and astructure that seals the cavity by bonding the second substrate to thefirst substrate.
 2. The device of claim 1, further comprising anelectronic bandgap structure on the insulative layer.
 3. The device ofclaim 1, wherein the cavity contains dipolar molecules.
 4. The device ofclaim 3, wherein the dipolar molecules are water molecules, and thecavity has a pressure of less than 0.15 mbars.
 5. The device of claim 1,wherein the insulative layer includes at least one of glass, ceramic or,silicon.
 6. The device of claim 1, wherein: the first substrate includesat least one of a semiconductor wafer, a ceramic or a metal; and thesecond substrate includes at least one of a semiconductor wafer, aceramic or a metal.
 7. The device of claim 1, wherein the insulativelayer includes glass, the first substrate includes a first semiconductorwafer, and the second substrate includes a second semiconductor wafer.8. The device of claim 1, wherein: the antenna is a first antenna; thedevice includes an amplifier, a filter, a signal generator, and a secondantenna on the insulative layer; the signal generator is coupled to thefirst antenna and is configured to generate a transmit signal to thefirst antenna; the amplifier is coupled to the second antenna and isconfigured to generate an error signal based on a receive signal fromthe second antenna and the transmit signal; and the filter is coupled tothe amplifier and to the signal generator, and is configured to generatea control output signal, based on the error signal, to adjust afrequency of the transmit signal generated by the signal generator. 9.The device of claim 1, wherein the metal layer is a first metal layer,and the bonding structure includes a second metal layer.
 10. A device,comprising: a first semiconductor substrate having opposite first andsecond sides, a cavity extending from the second side of the firstsemiconductor substrate through the first semiconductor substrate to thefirst side of the first semiconductor substrate; a first oxide layer onthe first side of the first semiconductor substrate; a metal layer onthe first oxide layer; a second oxide layer on the metal layer, thecavity extending from the first side of the first semiconductorsubstrate through the first oxide layer and through the metal layer tothe second oxide layer; a glass sheet on the second oxide layer; firstand second antennas on the glass sheet; a second semiconductorsubstrate; a structure that seals the cavity by bonding the secondsemiconductor substrate to the first semiconductor substrate; and atransceiver electrically coupled to the first and second antennas, thetransceiver configured to inject a transmit signal into the cavitythrough the first antenna, generate an error signal based on a receivesignal from the second antenna and the transmit signal, and dynamicallyadjust a frequency of the transmit signal based on the error signal; thecavity containing dipolar molecules and having an internal pressure ofless than 0.15 mbars.
 11. The device of claim 10, wherein thetransceiver includes: a signal generator coupled to the first antenna,the signal generator configured to generate the transmit signal; anamplifier coupled to the second antenna, the amplifier configured togenerate the error signal; and a loop filter coupled to the amplifierand to the signal generator, the loop filter configured to generate acontrol output signal to the signal generator based on the error signal.12. The device of claim 10, wherein the metal layer is a first metallayer, and the bonding structure includes a second metal layer.